Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270103020432/av1146sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270103020432/av1146Isup2.hkl |
CCDC reference: 226095
In a typical reaction, the dppb ligand (0.071 g, 0.17 mmol) in ethanol (30 ml) was slowly added to a solution of [Ru(tripod)Cl3] (0.125 g, 0.15 mmol) in acetontrile (150 ml). The mixture was refluxed for 3 h, during which time the initially deep-green solution gradually changed to yellow. After removal of the solvent, 5 drops of a saturated solution of NH4PF6 in ethanol were added to precipitate the products. The precipitate was filtered, washed with diethyl ether (2 × 10 ml) and dried under vacuum to give (I) as a yellow crystalline solid. Single crystals suitable for an X-ray structure determination were obtained by crystallization from acetone.
H atoms were treated as riding, with C—H distances in the range 0.93–0.97 Å and an O—H distance of 0.82 Å, and with Uiso(H) = 1.2Ueq(C) or 1.5Ueq(O). Please check this added text.
Data collection: IPDS (Stoe & Cie, 1997); cell refinement: IPDS; data reduction: IPDS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1996).
[Ru2Cl3(C41H39P3)2]PF6·C2H6O | F(000) = 3576 |
Mr = 1748.79 | Dx = 1.512 Mg m−3 |
Monoclinic, Cc | Melting point: 443 K |
Hall symbol: C -2yc | Mo Kα radiation, λ = 0.71073 Å |
a = 13.069 (3) Å | Cell parameters from 5000 reflections |
b = 25.602 (5) Å | θ = 1.8–25.9° |
c = 22.991 (5) Å | µ = 0.71 mm−1 |
β = 92.66 (3)° | T = 293 K |
V = 7684 (3) Å3 | Block, yellow |
Z = 4 | 0.20 × 0.12 × 0.09 mm |
Stoe IPDS area-detector diffractometer | 14149 independent reflections |
Radiation source: sealed tube | 11740 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
ϕ scans | θmax = 25.9°, θmin = 1.8° |
Absorption correction: numerical (X-RED; Stoe & Cie, 1997) | h = −15→16 |
Tmin = 0.908, Tmax = 0.959 | k = −31→31 |
26982 measured reflections | l = −28→26 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.033 | H-atom parameters constrained |
wR(F2) = 0.057 | w = 1/[σ2(Fo2) + (0.0176P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.89 | (Δ/σ)max = 0.001 |
14149 reflections | Δρmax = 0.39 e Å−3 |
933 parameters | Δρmin = −0.59 e Å−3 |
3 restraints | Absolute structure: Flack (1983), with 6746 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.725 (17) |
[Ru2Cl3(C41H39P3)2]PF6·C2H6O | V = 7684 (3) Å3 |
Mr = 1748.79 | Z = 4 |
Monoclinic, Cc | Mo Kα radiation |
a = 13.069 (3) Å | µ = 0.71 mm−1 |
b = 25.602 (5) Å | T = 293 K |
c = 22.991 (5) Å | 0.20 × 0.12 × 0.09 mm |
β = 92.66 (3)° |
Stoe IPDS area-detector diffractometer | 14149 independent reflections |
Absorption correction: numerical (X-RED; Stoe & Cie, 1997) | 11740 reflections with I > 2σ(I) |
Tmin = 0.908, Tmax = 0.959 | Rint = 0.039 |
26982 measured reflections |
R[F2 > 2σ(F2)] = 0.033 | H-atom parameters constrained |
wR(F2) = 0.057 | Δρmax = 0.39 e Å−3 |
S = 0.89 | Δρmin = −0.59 e Å−3 |
14149 reflections | Absolute structure: Flack (1983), with 6746 Friedel pairs |
933 parameters | Absolute structure parameter: 0.725 (17) |
3 restraints |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were generated with HFIX. Temperature factors U(H) = 1.2 U(C) for CH and CH2, 1.5 U(C,O) for CH3 and OH. The structure was refined as a racemic twin and yields a volume ratio of 0.725: 0.275. |
x | y | z | Uiso*/Ueq | ||
Ru1 | 0.90716 (2) | 0.101994 (11) | 0.299378 (14) | 0.01444 (7) | |
Ru2 | 0.83548 (2) | 0.204760 (11) | 0.213142 (13) | 0.01618 (7) | |
Cl1 | 0.97385 (9) | 0.13916 (4) | 0.20977 (5) | 0.0333 (3) | |
Cl2 | 0.74810 (8) | 0.12432 (4) | 0.24390 (5) | 0.0294 (2) | |
Cl3 | 0.89236 (8) | 0.19581 (4) | 0.31697 (4) | 0.0300 (2) | |
P1 | 0.84146 (7) | 0.08406 (4) | 0.38574 (4) | 0.0177 (2) | |
P2 | 0.89468 (7) | 0.01497 (4) | 0.28107 (4) | 0.0164 (2) | |
P3 | 1.06636 (7) | 0.08545 (4) | 0.33854 (4) | 0.0177 (2) | |
P4 | 0.68196 (8) | 0.24561 (4) | 0.21222 (4) | 0.0181 (2) | |
P5 | 0.82749 (8) | 0.20699 (4) | 0.11452 (4) | 0.0203 (2) | |
P6 | 0.91334 (8) | 0.28366 (4) | 0.21085 (4) | 0.0193 (2) | |
P7 | 0.31361 (9) | 0.01463 (5) | 0.01538 (5) | 0.0363 (3) | |
F1 | 0.4256 (2) | 0.03052 (13) | 0.00022 (15) | 0.0662 (9) | |
F2 | 0.2726 (2) | 0.03213 (13) | −0.04727 (14) | 0.0654 (9) | |
F3 | 0.2953 (3) | 0.07073 (16) | 0.0385 (2) | 0.1154 (17) | |
F4 | 0.3330 (3) | −0.04211 (12) | −0.00917 (15) | 0.0724 (10) | |
F5 | 0.2020 (2) | −0.00248 (18) | 0.03012 (16) | 0.0929 (13) | |
F6 | 0.3545 (3) | −0.00436 (17) | 0.07785 (13) | 0.0831 (12) | |
O1 | 0.9653 (3) | 0.37704 (16) | 0.03907 (19) | 0.0713 (12) | |
H1 | 0.9548 | 0.3495 | 0.0215 | 0.107* | |
C1A | 1.0686 (4) | 0.3861 (2) | 0.0446 (2) | 0.0569 (15) | |
H1AA | 1.0964 | 0.3864 | 0.0062 | 0.068* | |
H1AB | 1.1010 | 0.3578 | 0.0666 | 0.068* | |
C1 | 0.9824 (3) | −0.00164 (15) | 0.39652 (16) | 0.0200 (9) | |
C2A | 1.0943 (5) | 0.4364 (2) | 0.0743 (3) | 0.0742 (18) | |
H2AC | 1.0812 | 0.4648 | 0.0477 | 0.089* | |
H2AB | 1.1654 | 0.4364 | 0.0869 | 0.089* | |
H2AA | 1.0530 | 0.4404 | 0.1074 | 0.089* | |
C2 | 1.0132 (3) | −0.04669 (16) | 0.43697 (19) | 0.0297 (10) | |
H2A | 1.0747 | −0.0626 | 0.4240 | 0.036* | |
H2B | 0.9592 | −0.0721 | 0.4365 | 0.036* | |
H2C | 1.0252 | −0.0337 | 0.4759 | 0.036* | |
C3 | 0.9728 (3) | −0.02418 (14) | 0.33356 (16) | 0.0191 (8) | |
H3A | 0.9433 | −0.0589 | 0.3353 | 0.023* | |
H3B | 1.0410 | −0.0277 | 0.3191 | 0.023* | |
C4 | 1.0656 (3) | 0.04056 (15) | 0.40147 (16) | 0.0218 (9) | |
H4A | 1.1319 | 0.0237 | 0.4058 | 0.026* | |
H4B | 1.0560 | 0.0609 | 0.4364 | 0.026* | |
C5 | 0.8789 (3) | 0.01990 (14) | 0.41624 (16) | 0.0199 (9) | |
H5A | 0.8823 | 0.0226 | 0.4584 | 0.024* | |
H5B | 0.8256 | −0.0051 | 0.4055 | 0.024* | |
C6 | 0.7581 (3) | 0.31442 (15) | 0.12339 (18) | 0.0238 (10) | |
C7 | 0.7722 (3) | 0.26783 (15) | 0.08220 (17) | 0.0255 (9) | |
H7A | 0.8159 | 0.2791 | 0.0516 | 0.031* | |
H7B | 0.7059 | 0.2594 | 0.0640 | 0.031* | |
C8 | 0.8588 (3) | 0.32969 (15) | 0.15548 (17) | 0.0253 (9) | |
H8A | 0.8484 | 0.3630 | 0.1744 | 0.030* | |
H8B | 0.9095 | 0.3351 | 0.1266 | 0.030* | |
C9 | 0.6715 (3) | 0.30444 (13) | 0.16498 (17) | 0.0235 (9) | |
H9A | 0.6077 | 0.3020 | 0.1418 | 0.028* | |
H9B | 0.6665 | 0.3348 | 0.1900 | 0.028* | |
C10 | 0.7237 (4) | 0.36121 (16) | 0.08515 (19) | 0.0325 (11) | |
H10A | 0.7776 | 0.3706 | 0.0601 | 0.039* | |
H10B | 0.7086 | 0.3904 | 0.1096 | 0.039* | |
H10C | 0.6635 | 0.3519 | 0.0619 | 0.039* | |
C11A | 0.7013 (3) | 0.08610 (15) | 0.38720 (16) | 0.0212 (9) | |
C11B | 0.8720 (3) | 0.12824 (15) | 0.44801 (16) | 0.0223 (9) | |
C12A | 0.6562 (3) | 0.13493 (18) | 0.37883 (18) | 0.0316 (10) | |
H12A | 0.6970 | 0.1639 | 0.3723 | 0.038* | |
C12B | 0.8198 (4) | 0.12136 (18) | 0.49782 (18) | 0.0346 (11) | |
H12B | 0.7735 | 0.0939 | 0.4997 | 0.042* | |
C13A | 0.5515 (3) | 0.1408 (2) | 0.3802 (2) | 0.0396 (12) | |
H13A | 0.5220 | 0.1736 | 0.3754 | 0.048* | |
C13B | 0.8338 (4) | 0.1538 (2) | 0.5447 (2) | 0.0450 (13) | |
H13B | 0.7959 | 0.1488 | 0.5774 | 0.054* | |
C14A | 0.4903 (3) | 0.0975 (2) | 0.3887 (2) | 0.0424 (12) | |
H14A | 0.4195 | 0.1011 | 0.3886 | 0.051* | |
C14B | 0.9031 (4) | 0.1934 (2) | 0.5437 (2) | 0.0473 (13) | |
H14B | 0.9115 | 0.2159 | 0.5753 | 0.057* | |
C15A | 0.5344 (3) | 0.0496 (2) | 0.3971 (2) | 0.0426 (13) | |
H15A | 0.4931 | 0.0207 | 0.4032 | 0.051* | |
C15B | 0.9602 (4) | 0.1998 (2) | 0.4958 (2) | 0.0481 (14) | |
H15B | 1.0100 | 0.2257 | 0.4955 | 0.058* | |
C16A | 0.6388 (3) | 0.04338 (17) | 0.39657 (19) | 0.0299 (10) | |
H16A | 0.6676 | 0.0105 | 0.4025 | 0.036* | |
C16B | 0.9435 (4) | 0.16731 (18) | 0.4473 (2) | 0.0366 (12) | |
H16B | 0.9812 | 0.1723 | 0.4144 | 0.044* | |
C21A | 0.9268 (3) | −0.00966 (15) | 0.20933 (16) | 0.0222 (9) | |
C21B | 0.7674 (3) | −0.01477 (14) | 0.28391 (16) | 0.0193 (8) | |
C22A | 0.9703 (3) | −0.05854 (16) | 0.20211 (19) | 0.0320 (10) | |
H22A | 0.9850 | −0.0798 | 0.2342 | 0.038* | |
C22B | 0.7441 (3) | −0.05770 (16) | 0.31862 (19) | 0.0321 (10) | |
H22B | 0.7957 | −0.0730 | 0.3421 | 0.039* | |
C23A | 0.9916 (4) | −0.0753 (2) | 0.1467 (2) | 0.0494 (14) | |
H23A | 1.0215 | −0.1079 | 0.1418 | 0.059* | |
C23B | 0.6474 (4) | −0.0774 (2) | 0.3186 (2) | 0.0427 (12) | |
H23B | 0.6339 | −0.1058 | 0.3424 | 0.051* | |
C24A | 0.9691 (4) | −0.0446 (2) | 0.0992 (2) | 0.0481 (14) | |
H24A | 0.9859 | −0.0557 | 0.0623 | 0.058* | |
C24B | 0.5696 (4) | −0.0562 (2) | 0.2843 (3) | 0.0470 (14) | |
H24B | 0.5035 | −0.0694 | 0.2858 | 0.056* | |
C25A | 0.9226 (4) | 0.00182 (19) | 0.1060 (2) | 0.0436 (13) | |
H25A | 0.9042 | 0.0220 | 0.0736 | 0.052* | |
C25B | 0.5894 (3) | −0.0163 (2) | 0.2484 (2) | 0.0452 (13) | |
H25B | 0.5369 | −0.0023 | 0.2245 | 0.054* | |
C26A | 0.9018 (3) | 0.01968 (17) | 0.16111 (17) | 0.0308 (10) | |
H26A | 0.8706 | 0.0520 | 0.1653 | 0.037* | |
C26B | 0.6893 (3) | 0.00458 (18) | 0.2468 (2) | 0.0373 (11) | |
H26B | 0.7029 | 0.0313 | 0.2210 | 0.045* | |
C31A | 1.1484 (3) | 0.13973 (15) | 0.36416 (17) | 0.0215 (9) | |
C31B | 1.1597 (3) | 0.05372 (14) | 0.29157 (17) | 0.0201 (9) | |
C32A | 1.2091 (3) | 0.13792 (17) | 0.41579 (18) | 0.0295 (10) | |
H32A | 1.2033 | 0.1100 | 0.4413 | 0.035* | |
C32B | 1.1420 (3) | 0.04843 (19) | 0.23168 (19) | 0.0334 (11) | |
H32B | 1.0810 | 0.0604 | 0.2140 | 0.040* | |
C33A | 1.2772 (4) | 0.17752 (18) | 0.42868 (19) | 0.0359 (11) | |
H33A | 1.3184 | 0.1758 | 0.4627 | 0.043* | |
C33B | 1.2149 (4) | 0.0254 (2) | 0.1986 (2) | 0.0467 (13) | |
H33B | 1.2027 | 0.0224 | 0.1586 | 0.056* | |
C34A | 1.2857 (4) | 0.21958 (18) | 0.3922 (2) | 0.0412 (12) | |
H34A | 1.3314 | 0.2464 | 0.4016 | 0.049* | |
C34B | 1.3029 (4) | 0.0071 (2) | 0.2230 (2) | 0.0490 (14) | |
H34B | 1.3507 | −0.0090 | 0.2002 | 0.059* | |
C35A | 1.2259 (4) | 0.22149 (19) | 0.3418 (2) | 0.0470 (13) | |
H35A | 1.2314 | 0.2499 | 0.3169 | 0.056* | |
C35B | 1.3216 (4) | 0.0125 (2) | 0.2811 (2) | 0.0471 (13) | |
H35B | 1.3833 | 0.0007 | 0.2981 | 0.057* | |
C36A | 1.1583 (3) | 0.18237 (17) | 0.3276 (2) | 0.0360 (11) | |
H36A | 1.1184 | 0.1843 | 0.2931 | 0.043* | |
C36B | 1.2510 (3) | 0.03505 (18) | 0.3153 (2) | 0.0343 (11) | |
H36B | 1.2650 | 0.0378 | 0.3552 | 0.041* | |
C41A | 0.6276 (3) | 0.27088 (15) | 0.27855 (18) | 0.0244 (9) | |
C41B | 0.5740 (3) | 0.20461 (16) | 0.18605 (18) | 0.0250 (9) | |
C42A | 0.6786 (4) | 0.26903 (17) | 0.33218 (18) | 0.0332 (11) | |
H42A | 0.7436 | 0.2543 | 0.3359 | 0.040* | |
C42B | 0.5277 (4) | 0.17226 (18) | 0.2259 (2) | 0.0402 (12) | |
H42B | 0.5502 | 0.1728 | 0.2648 | 0.048* | |
C43A | 0.6334 (5) | 0.2891 (2) | 0.3808 (2) | 0.0518 (14) | |
H43A | 0.6688 | 0.2874 | 0.4168 | 0.062* | |
C43B | 0.4486 (4) | 0.1394 (2) | 0.2080 (3) | 0.0516 (14) | |
H43B | 0.4186 | 0.1179 | 0.2351 | 0.062* | |
C44A | 0.5394 (5) | 0.31115 (19) | 0.3773 (2) | 0.0562 (16) | |
H44A | 0.5106 | 0.3248 | 0.4103 | 0.067* | |
C44B | 0.4135 (4) | 0.1378 (2) | 0.1506 (3) | 0.0531 (14) | |
H44B | 0.3611 | 0.1150 | 0.1387 | 0.064* | |
C45A | 0.4871 (5) | 0.3130 (2) | 0.3241 (3) | 0.0554 (15) | |
H45A | 0.4221 | 0.3278 | 0.3212 | 0.067* | |
C45B | 0.4565 (4) | 0.1701 (2) | 0.1113 (2) | 0.0440 (13) | |
H45B | 0.4322 | 0.1698 | 0.0726 | 0.053* | |
C46A | 0.5299 (3) | 0.29332 (19) | 0.2750 (2) | 0.0418 (12) | |
H46A | 0.4936 | 0.2950 | 0.2393 | 0.050* | |
C46B | 0.5371 (3) | 0.20363 (18) | 0.12878 (19) | 0.0343 (10) | |
H46B | 0.5659 | 0.2254 | 0.1016 | 0.041* | |
C51A | 0.9522 (3) | 0.20103 (17) | 0.08136 (16) | 0.0262 (9) | |
C51B | 0.7578 (3) | 0.15728 (16) | 0.07079 (18) | 0.0273 (10) | |
C52A | 0.9963 (3) | 0.15151 (18) | 0.0781 (2) | 0.0344 (11) | |
H52A | 0.9603 | 0.1226 | 0.0904 | 0.041* | |
C52B | 0.7042 (4) | 0.11782 (17) | 0.0952 (2) | 0.0415 (12) | |
H52B | 0.7032 | 0.1146 | 0.1355 | 0.050* | |
C53A | 1.0910 (4) | 0.1448 (2) | 0.0571 (2) | 0.0442 (13) | |
H53A | 1.1190 | 0.1115 | 0.0555 | 0.053* | |
C53B | 0.6508 (4) | 0.0823 (2) | 0.0589 (3) | 0.0617 (17) | |
H53B | 0.6133 | 0.0556 | 0.0752 | 0.074* | |
C54A | 1.1452 (4) | 0.1866 (2) | 0.0386 (2) | 0.0470 (14) | |
H54A | 1.2108 | 0.1821 | 0.0255 | 0.056* | |
C54B | 0.6529 (5) | 0.0863 (3) | 0.0002 (3) | 0.0649 (17) | |
H54B | 0.6163 | 0.0626 | −0.0234 | 0.078* | |
C55A | 1.1030 (4) | 0.2349 (2) | 0.0396 (2) | 0.0461 (13) | |
H55A | 1.1393 | 0.2629 | 0.0252 | 0.055* | |
C55B | 0.7074 (5) | 0.1241 (3) | −0.0239 (3) | 0.0694 (18) | |
H55B | 0.7103 | 0.1259 | −0.0642 | 0.083* | |
C56A | 1.0066 (3) | 0.24368 (17) | 0.06150 (18) | 0.0322 (10) | |
H56A | 0.9794 | 0.2772 | 0.0628 | 0.039* | |
C56B | 0.7594 (4) | 0.1607 (2) | 0.0104 (2) | 0.0492 (13) | |
H56B | 0.7954 | 0.1875 | −0.0068 | 0.059* | |
C61A | 1.0518 (3) | 0.28902 (17) | 0.19975 (16) | 0.0266 (9) | |
C61B | 0.9073 (3) | 0.32007 (15) | 0.27978 (17) | 0.0248 (10) | |
C62A | 1.1137 (3) | 0.24683 (19) | 0.19267 (19) | 0.0386 (11) | |
H62A | 1.0867 | 0.2132 | 0.1919 | 0.046* | |
C62B | 0.9747 (4) | 0.30707 (17) | 0.32586 (18) | 0.0333 (11) | |
H62B | 1.0246 | 0.2818 | 0.3206 | 0.040* | |
C63A | 1.2194 (4) | 0.2551 (2) | 0.1865 (2) | 0.0533 (15) | |
H63A | 1.2626 | 0.2267 | 0.1820 | 0.064* | |
C63B | 0.9690 (4) | 0.3309 (2) | 0.3792 (2) | 0.0475 (14) | |
H63B | 1.0153 | 0.3219 | 0.4095 | 0.057* | |
C64A | 1.2591 (4) | 0.3050 (3) | 0.1872 (2) | 0.0593 (18) | |
H64A | 1.3289 | 0.3100 | 0.1832 | 0.071* | |
C64B | 0.8949 (5) | 0.3679 (2) | 0.3880 (2) | 0.0527 (16) | |
H64B | 0.8905 | 0.3834 | 0.4244 | 0.063* | |
C65A | 1.1973 (4) | 0.3463 (3) | 0.1934 (2) | 0.0536 (15) | |
H65A | 1.2241 | 0.3800 | 0.1938 | 0.064* | |
C65B | 0.8274 (4) | 0.38208 (18) | 0.3429 (2) | 0.0467 (14) | |
H65B | 0.7784 | 0.4077 | 0.3485 | 0.056* | |
C66A | 1.0948 (4) | 0.33857 (19) | 0.1992 (2) | 0.0401 (12) | |
H66A | 1.0525 | 0.3675 | 0.2029 | 0.048* | |
C66B | 0.8329 (4) | 0.35795 (17) | 0.2893 (2) | 0.0352 (11) | |
H66B | 0.7864 | 0.3671 | 0.2592 | 0.042* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ru1 | 0.01471 (15) | 0.01383 (14) | 0.01470 (14) | −0.00060 (14) | −0.00021 (12) | 0.00210 (13) |
Ru2 | 0.01867 (17) | 0.01274 (15) | 0.01687 (16) | 0.00091 (15) | −0.00185 (13) | 0.00067 (14) |
Cl1 | 0.0387 (6) | 0.0285 (6) | 0.0322 (6) | 0.0013 (5) | −0.0044 (5) | 0.0067 (5) |
Cl2 | 0.0320 (6) | 0.0230 (5) | 0.0328 (6) | 0.0029 (4) | −0.0037 (5) | 0.0025 (4) |
Cl3 | 0.0337 (6) | 0.0250 (5) | 0.0311 (6) | −0.0021 (5) | −0.0021 (5) | 0.0059 (4) |
P1 | 0.0176 (5) | 0.0186 (5) | 0.0169 (5) | −0.0015 (4) | 0.0019 (4) | 0.0017 (4) |
P2 | 0.0166 (5) | 0.0163 (5) | 0.0164 (5) | 0.0007 (4) | 0.0008 (4) | 0.0009 (4) |
P3 | 0.0165 (5) | 0.0196 (5) | 0.0168 (5) | −0.0019 (4) | −0.0013 (4) | 0.0031 (4) |
P4 | 0.0204 (5) | 0.0148 (5) | 0.0190 (5) | 0.0011 (4) | −0.0003 (4) | 0.0007 (4) |
P5 | 0.0233 (6) | 0.0179 (5) | 0.0196 (5) | 0.0014 (5) | −0.0020 (4) | −0.0013 (4) |
P6 | 0.0225 (5) | 0.0176 (5) | 0.0180 (5) | −0.0019 (4) | 0.0020 (4) | −0.0001 (4) |
P7 | 0.0305 (7) | 0.0469 (7) | 0.0312 (7) | 0.0028 (6) | −0.0018 (5) | −0.0073 (6) |
F1 | 0.0344 (17) | 0.077 (2) | 0.087 (3) | −0.0128 (16) | −0.0034 (16) | 0.0018 (19) |
F2 | 0.062 (2) | 0.078 (2) | 0.0545 (19) | −0.0260 (18) | −0.0248 (16) | 0.0264 (17) |
F3 | 0.113 (4) | 0.088 (3) | 0.142 (4) | 0.048 (3) | −0.030 (3) | −0.073 (3) |
F4 | 0.091 (3) | 0.0432 (18) | 0.083 (3) | −0.0047 (18) | 0.001 (2) | −0.0184 (17) |
F5 | 0.0322 (18) | 0.171 (4) | 0.076 (2) | −0.002 (2) | 0.0100 (17) | 0.039 (3) |
F6 | 0.063 (2) | 0.145 (3) | 0.0396 (19) | 0.023 (2) | −0.0137 (16) | 0.008 (2) |
O1 | 0.067 (3) | 0.065 (3) | 0.082 (3) | −0.013 (2) | 0.005 (2) | 0.014 (2) |
C1A | 0.049 (4) | 0.070 (4) | 0.052 (3) | −0.004 (3) | 0.011 (3) | 0.005 (3) |
C1 | 0.020 (2) | 0.022 (2) | 0.018 (2) | −0.0041 (18) | −0.0016 (16) | 0.0066 (17) |
C2A | 0.076 (5) | 0.060 (4) | 0.086 (5) | 0.008 (4) | −0.004 (4) | −0.007 (4) |
C2 | 0.031 (2) | 0.027 (2) | 0.030 (2) | 0.000 (2) | −0.001 (2) | 0.0088 (19) |
C3 | 0.018 (2) | 0.0168 (19) | 0.022 (2) | 0.0029 (16) | −0.0012 (16) | 0.0043 (16) |
C4 | 0.023 (2) | 0.028 (2) | 0.0140 (19) | 0.0028 (18) | −0.0011 (16) | 0.0067 (17) |
C5 | 0.023 (2) | 0.017 (2) | 0.019 (2) | −0.0012 (17) | 0.0017 (17) | 0.0069 (16) |
C6 | 0.027 (2) | 0.022 (2) | 0.023 (2) | 0.0076 (18) | 0.0060 (18) | 0.0059 (18) |
C7 | 0.026 (2) | 0.027 (2) | 0.023 (2) | 0.0059 (18) | −0.0043 (18) | 0.0047 (18) |
C8 | 0.034 (3) | 0.0175 (19) | 0.025 (2) | −0.0011 (18) | 0.0091 (19) | 0.0060 (17) |
C9 | 0.028 (2) | 0.0123 (19) | 0.030 (2) | 0.0053 (17) | 0.0005 (18) | 0.0024 (16) |
C10 | 0.037 (3) | 0.028 (2) | 0.033 (3) | 0.008 (2) | 0.003 (2) | 0.008 (2) |
C11A | 0.017 (2) | 0.031 (2) | 0.0155 (19) | 0.0015 (17) | 0.0041 (16) | 0.0021 (16) |
C11B | 0.024 (2) | 0.024 (2) | 0.019 (2) | 0.0012 (18) | −0.0023 (17) | −0.0054 (17) |
C12A | 0.029 (3) | 0.036 (3) | 0.031 (2) | 0.002 (2) | 0.006 (2) | 0.008 (2) |
C12B | 0.045 (3) | 0.038 (3) | 0.022 (2) | −0.014 (2) | 0.006 (2) | 0.0001 (19) |
C13A | 0.031 (3) | 0.047 (3) | 0.041 (3) | 0.013 (2) | 0.006 (2) | 0.012 (2) |
C13B | 0.050 (3) | 0.056 (3) | 0.029 (3) | −0.011 (3) | 0.006 (2) | −0.016 (2) |
C14A | 0.018 (2) | 0.067 (4) | 0.043 (3) | 0.001 (3) | 0.004 (2) | −0.004 (3) |
C14B | 0.051 (3) | 0.058 (4) | 0.033 (3) | −0.005 (3) | 0.004 (2) | −0.022 (2) |
C15A | 0.028 (3) | 0.057 (3) | 0.045 (3) | −0.013 (2) | 0.016 (2) | −0.008 (3) |
C15B | 0.048 (3) | 0.047 (3) | 0.049 (3) | −0.019 (3) | 0.002 (3) | −0.015 (3) |
C16A | 0.022 (2) | 0.031 (2) | 0.037 (3) | −0.001 (2) | 0.005 (2) | −0.003 (2) |
C16B | 0.038 (3) | 0.038 (3) | 0.034 (3) | −0.005 (2) | 0.009 (2) | −0.010 (2) |
C21A | 0.022 (2) | 0.024 (2) | 0.020 (2) | 0.0005 (17) | 0.0009 (17) | −0.0020 (17) |
C21B | 0.017 (2) | 0.018 (2) | 0.023 (2) | −0.0060 (16) | 0.0024 (17) | −0.0040 (16) |
C22A | 0.041 (3) | 0.027 (2) | 0.028 (2) | 0.010 (2) | 0.003 (2) | −0.0003 (19) |
C22B | 0.033 (3) | 0.027 (2) | 0.035 (3) | −0.013 (2) | 0.000 (2) | −0.003 (2) |
C23A | 0.061 (4) | 0.048 (3) | 0.040 (3) | 0.026 (3) | 0.006 (3) | −0.015 (2) |
C23B | 0.041 (3) | 0.045 (3) | 0.042 (3) | −0.020 (2) | 0.002 (2) | −0.003 (2) |
C24A | 0.061 (4) | 0.059 (4) | 0.025 (3) | 0.014 (3) | 0.009 (2) | −0.011 (2) |
C24B | 0.031 (3) | 0.041 (3) | 0.070 (4) | −0.020 (2) | 0.013 (3) | −0.025 (3) |
C25A | 0.071 (4) | 0.040 (3) | 0.020 (2) | 0.002 (3) | 0.003 (2) | −0.003 (2) |
C25B | 0.018 (2) | 0.052 (3) | 0.065 (4) | 0.006 (2) | −0.010 (2) | −0.009 (3) |
C26A | 0.042 (3) | 0.029 (2) | 0.022 (2) | 0.010 (2) | 0.002 (2) | −0.0022 (19) |
C26B | 0.023 (2) | 0.038 (3) | 0.051 (3) | −0.003 (2) | 0.000 (2) | −0.001 (2) |
C31A | 0.0124 (19) | 0.026 (2) | 0.026 (2) | −0.0071 (16) | −0.0010 (16) | −0.0026 (17) |
C31B | 0.013 (2) | 0.021 (2) | 0.027 (2) | −0.0009 (16) | 0.0037 (17) | 0.0039 (17) |
C32A | 0.036 (3) | 0.031 (2) | 0.021 (2) | −0.006 (2) | −0.0035 (19) | −0.0023 (18) |
C32B | 0.018 (2) | 0.061 (3) | 0.021 (2) | −0.004 (2) | 0.0013 (19) | 0.005 (2) |
C33A | 0.039 (3) | 0.045 (3) | 0.023 (2) | −0.006 (2) | −0.004 (2) | −0.011 (2) |
C33B | 0.036 (3) | 0.080 (4) | 0.024 (2) | −0.016 (3) | 0.010 (2) | −0.014 (3) |
C34A | 0.041 (3) | 0.042 (3) | 0.041 (3) | −0.015 (2) | 0.001 (2) | −0.009 (2) |
C34B | 0.031 (3) | 0.065 (4) | 0.053 (3) | −0.004 (3) | 0.020 (3) | −0.014 (3) |
C35A | 0.051 (3) | 0.038 (3) | 0.051 (3) | −0.021 (2) | −0.012 (3) | 0.013 (2) |
C35B | 0.028 (3) | 0.062 (4) | 0.052 (3) | 0.014 (2) | 0.005 (2) | 0.000 (3) |
C36A | 0.036 (3) | 0.034 (3) | 0.037 (3) | −0.015 (2) | −0.013 (2) | 0.015 (2) |
C36B | 0.029 (3) | 0.043 (3) | 0.031 (2) | 0.010 (2) | 0.001 (2) | −0.001 (2) |
C41A | 0.028 (2) | 0.018 (2) | 0.029 (2) | −0.0029 (18) | 0.0088 (19) | −0.0012 (17) |
C41B | 0.018 (2) | 0.020 (2) | 0.037 (2) | 0.0053 (18) | −0.0053 (17) | 0.0012 (19) |
C42A | 0.038 (3) | 0.032 (2) | 0.030 (3) | −0.002 (2) | 0.008 (2) | 0.003 (2) |
C42B | 0.036 (3) | 0.035 (3) | 0.049 (3) | −0.012 (2) | 0.001 (2) | 0.003 (2) |
C43A | 0.075 (4) | 0.054 (3) | 0.028 (3) | −0.019 (3) | 0.012 (3) | −0.002 (2) |
C43B | 0.040 (3) | 0.043 (3) | 0.071 (4) | −0.019 (3) | −0.006 (3) | 0.008 (3) |
C44A | 0.082 (5) | 0.036 (3) | 0.054 (4) | −0.012 (3) | 0.041 (3) | −0.015 (3) |
C44B | 0.038 (3) | 0.044 (3) | 0.075 (4) | −0.013 (3) | −0.017 (3) | −0.010 (3) |
C45A | 0.054 (3) | 0.046 (3) | 0.069 (4) | 0.012 (3) | 0.031 (3) | −0.002 (3) |
C45B | 0.036 (3) | 0.043 (3) | 0.051 (3) | −0.004 (2) | −0.020 (2) | −0.014 (3) |
C46A | 0.033 (3) | 0.044 (3) | 0.049 (3) | 0.013 (2) | 0.010 (2) | 0.000 (2) |
C46B | 0.036 (3) | 0.035 (2) | 0.032 (2) | 0.003 (2) | −0.006 (2) | 0.001 (2) |
C51A | 0.027 (2) | 0.033 (2) | 0.019 (2) | 0.003 (2) | 0.0040 (17) | −0.0048 (18) |
C51B | 0.024 (2) | 0.027 (2) | 0.030 (2) | −0.0003 (18) | −0.0066 (19) | −0.0136 (19) |
C52A | 0.035 (3) | 0.030 (3) | 0.038 (3) | 0.007 (2) | 0.003 (2) | 0.001 (2) |
C52B | 0.049 (3) | 0.031 (3) | 0.045 (3) | 0.002 (2) | 0.001 (2) | −0.017 (2) |
C53A | 0.040 (3) | 0.046 (3) | 0.047 (3) | 0.024 (3) | 0.007 (2) | −0.006 (3) |
C53B | 0.057 (4) | 0.038 (3) | 0.090 (5) | −0.018 (3) | −0.003 (3) | −0.020 (3) |
C54A | 0.032 (3) | 0.075 (4) | 0.035 (3) | 0.013 (3) | 0.011 (2) | −0.002 (3) |
C54B | 0.053 (4) | 0.069 (4) | 0.072 (4) | −0.002 (3) | −0.008 (3) | −0.044 (4) |
C55A | 0.052 (3) | 0.053 (3) | 0.036 (3) | −0.006 (3) | 0.019 (2) | 0.006 (2) |
C55B | 0.062 (4) | 0.099 (5) | 0.046 (3) | 0.002 (4) | −0.013 (3) | −0.032 (3) |
C56A | 0.037 (3) | 0.033 (2) | 0.027 (2) | 0.001 (2) | 0.006 (2) | −0.0027 (19) |
C56B | 0.058 (3) | 0.058 (3) | 0.031 (3) | −0.006 (3) | −0.010 (2) | −0.013 (2) |
C61A | 0.021 (2) | 0.043 (3) | 0.016 (2) | −0.002 (2) | 0.0012 (16) | −0.0011 (19) |
C61B | 0.031 (2) | 0.022 (2) | 0.022 (2) | −0.0162 (19) | 0.011 (2) | −0.0025 (17) |
C62A | 0.034 (3) | 0.049 (3) | 0.033 (3) | 0.003 (2) | −0.002 (2) | 0.005 (2) |
C62B | 0.042 (3) | 0.032 (3) | 0.026 (2) | −0.016 (2) | 0.004 (2) | 0.0001 (19) |
C63A | 0.035 (3) | 0.084 (4) | 0.041 (3) | 0.027 (3) | 0.004 (2) | 0.005 (3) |
C63B | 0.061 (4) | 0.056 (3) | 0.026 (3) | −0.034 (3) | 0.001 (2) | −0.004 (2) |
C64A | 0.029 (3) | 0.119 (6) | 0.030 (3) | −0.018 (4) | 0.001 (2) | 0.019 (3) |
C64B | 0.082 (4) | 0.043 (3) | 0.036 (3) | −0.032 (3) | 0.024 (3) | −0.021 (3) |
C65A | 0.032 (3) | 0.088 (4) | 0.041 (3) | −0.020 (3) | 0.007 (2) | −0.004 (3) |
C65B | 0.058 (4) | 0.028 (3) | 0.056 (3) | −0.015 (2) | 0.029 (3) | −0.019 (2) |
C66A | 0.036 (3) | 0.045 (3) | 0.040 (3) | −0.016 (2) | 0.009 (2) | −0.009 (2) |
C66B | 0.042 (3) | 0.027 (2) | 0.038 (3) | −0.012 (2) | 0.016 (2) | −0.012 (2) |
Ru1—P1 | 2.2469 (11) | C23A—H23A | 0.9300 |
Ru1—P3 | 2.2682 (12) | C23B—C24B | 1.369 (7) |
Ru1—P2 | 2.2719 (11) | C23B—H23B | 0.9300 |
Ru1—Cl3 | 2.4449 (12) | C24A—C25A | 1.348 (7) |
Ru1—Cl2 | 2.4553 (13) | C24A—H24A | 0.9300 |
Ru1—Cl1 | 2.4650 (12) | C24B—C25B | 1.348 (7) |
Ru1—Ru2 | 3.3997 (7) | C24B—H24B | 0.9300 |
Ru2—P4 | 2.2617 (12) | C25A—C26A | 1.385 (6) |
Ru2—P6 | 2.2635 (11) | C25A—H25A | 0.9300 |
Ru2—P5 | 2.2657 (11) | C25B—C26B | 1.413 (6) |
Ru2—Cl1 | 2.4717 (12) | C25B—H25B | 0.9300 |
Ru2—Cl2 | 2.4738 (11) | C26A—H26A | 0.9300 |
Ru2—Cl3 | 2.4776 (12) | C26B—H26B | 0.9300 |
P1—C11A | 1.835 (4) | C31A—C36A | 1.387 (5) |
P1—C5 | 1.843 (4) | C31A—C32A | 1.397 (6) |
P1—C11B | 1.853 (4) | C31B—C36B | 1.374 (6) |
P2—C21A | 1.833 (4) | C31B—C32B | 1.392 (6) |
P2—C21B | 1.834 (4) | C32A—C33A | 1.373 (6) |
P2—C3 | 1.841 (4) | C32A—H32A | 0.9300 |
P3—C31A | 1.836 (4) | C32B—C33B | 1.379 (6) |
P3—C4 | 1.848 (4) | C32B—H32B | 0.9300 |
P3—C31B | 1.854 (4) | C33A—C34A | 1.372 (6) |
P4—C41A | 1.830 (4) | C33A—H33A | 0.9300 |
P4—C41B | 1.837 (4) | C33B—C34B | 1.340 (7) |
P4—C9 | 1.858 (4) | C33B—H33B | 0.9300 |
P5—C51B | 1.837 (4) | C34A—C35A | 1.368 (7) |
P5—C51A | 1.837 (4) | C34A—H34A | 0.9300 |
P5—C7 | 1.857 (4) | C34B—C35B | 1.355 (7) |
P6—C61B | 1.844 (4) | C34B—H34B | 0.9300 |
P6—C61A | 1.845 (4) | C35A—C36A | 1.365 (6) |
P6—C8 | 1.853 (4) | C35A—H35A | 0.9300 |
P7—F3 | 1.554 (4) | C35B—C36B | 1.366 (6) |
P7—F1 | 1.574 (3) | C35B—H35B | 0.9300 |
P7—F5 | 1.575 (3) | C36A—H36A | 0.9300 |
P7—F2 | 1.578 (3) | C36B—H36B | 0.9300 |
P7—F4 | 1.583 (3) | C41A—C42A | 1.375 (6) |
P7—F6 | 1.585 (3) | C41A—C46A | 1.399 (6) |
O1—C1A | 1.371 (6) | C41B—C46B | 1.381 (6) |
O1—H1 | 0.8200 | C41B—C42B | 1.394 (6) |
C1A—C2A | 1.487 (8) | C42A—C43A | 1.387 (6) |
C1A—H1AA | 0.9700 | C42A—H42A | 0.9300 |
C1A—H1AB | 0.9700 | C42B—C43B | 1.381 (6) |
C1—C2 | 1.524 (5) | C42B—H42B | 0.9300 |
C1—C4 | 1.533 (5) | C43A—C44A | 1.350 (8) |
C1—C5 | 1.549 (5) | C43A—H43A | 0.9300 |
C1—C3 | 1.558 (5) | C43B—C44B | 1.378 (8) |
C2A—H2AC | 0.9600 | C43B—H43B | 0.9300 |
C2A—H2AB | 0.9600 | C44A—C45A | 1.374 (8) |
C2A—H2AA | 0.9600 | C44A—H44A | 0.9300 |
C2—H2A | 0.9600 | C44B—C45B | 1.364 (7) |
C2—H2B | 0.9600 | C44B—H44B | 0.9300 |
C2—H2C | 0.9600 | C45A—C46A | 1.378 (7) |
C3—H3A | 0.9700 | C45A—H45A | 0.9300 |
C3—H3B | 0.9700 | C45B—C46B | 1.404 (6) |
C4—H4A | 0.9700 | C45B—H45B | 0.9300 |
C4—H4B | 0.9700 | C46A—H46A | 0.9300 |
C5—H5A | 0.9700 | C46B—H46B | 0.9300 |
C5—H5B | 0.9700 | C51A—C56A | 1.392 (6) |
C6—C8 | 1.529 (6) | C51A—C52A | 1.397 (6) |
C6—C9 | 1.536 (5) | C51B—C52B | 1.365 (6) |
C6—C7 | 1.539 (6) | C51B—C56B | 1.392 (6) |
C6—C10 | 1.541 (6) | C52A—C53A | 1.359 (6) |
C7—H7A | 0.9700 | C52A—H52A | 0.9300 |
C7—H7B | 0.9700 | C52B—C53B | 1.399 (7) |
C8—H8A | 0.9700 | C52B—H52B | 0.9300 |
C8—H8B | 0.9700 | C53A—C54A | 1.363 (7) |
C9—H9A | 0.9700 | C53A—H53A | 0.9300 |
C9—H9B | 0.9700 | C53B—C54B | 1.354 (8) |
C10—H10A | 0.9600 | C53B—H53B | 0.9300 |
C10—H10B | 0.9600 | C54A—C55A | 1.352 (7) |
C10—H10C | 0.9600 | C54A—H54A | 0.9300 |
C11A—C16A | 1.388 (6) | C54B—C55B | 1.339 (9) |
C11A—C12A | 1.392 (6) | C54B—H54B | 0.9300 |
C11B—C16B | 1.369 (6) | C55A—C56A | 1.398 (6) |
C11B—C12B | 1.371 (5) | C55A—H55A | 0.9300 |
C12A—C13A | 1.378 (6) | C55B—C56B | 1.384 (7) |
C12A—H12A | 0.9300 | C55B—H55B | 0.9300 |
C12B—C13B | 1.366 (6) | C56A—H56A | 0.9300 |
C12B—H12B | 0.9300 | C56B—H56B | 0.9300 |
C13A—C14A | 1.385 (7) | C61A—C62A | 1.363 (6) |
C13A—H13A | 0.9300 | C61A—C66A | 1.388 (6) |
C13B—C14B | 1.359 (7) | C61B—C62B | 1.387 (6) |
C13B—H13B | 0.9300 | C61B—C66B | 1.398 (6) |
C14A—C15A | 1.365 (7) | C62A—C63A | 1.412 (7) |
C14A—H14A | 0.9300 | C62A—H62A | 0.9300 |
C14B—C15B | 1.367 (7) | C62B—C63B | 1.374 (6) |
C14B—H14B | 0.9300 | C62B—H62B | 0.9300 |
C15A—C16A | 1.375 (6) | C63A—C64A | 1.378 (8) |
C15A—H15A | 0.9300 | C63A—H63A | 0.9300 |
C15B—C16B | 1.401 (6) | C63B—C64B | 1.376 (7) |
C15B—H15B | 0.9300 | C63B—H63B | 0.9300 |
C16A—H16A | 0.9300 | C64A—C65A | 1.343 (8) |
C16B—H16B | 0.9300 | C64A—H64A | 0.9300 |
C21A—C26A | 1.366 (6) | C64B—C65B | 1.378 (8) |
C21A—C22A | 1.388 (5) | C64B—H64B | 0.9300 |
C21B—C26B | 1.390 (6) | C65A—C66A | 1.367 (7) |
C21B—C22B | 1.400 (5) | C65A—H65A | 0.9300 |
C22A—C23A | 1.384 (6) | C65B—C66B | 1.383 (6) |
C22A—H22A | 0.9300 | C65B—H65B | 0.9300 |
C22B—C23B | 1.361 (6) | C66A—H66A | 0.9300 |
C22B—H22B | 0.9300 | C66B—H66B | 0.9300 |
C23A—C24A | 1.368 (7) | ||
P1—Ru1—P3 | 89.55 (4) | C14A—C15A—C16A | 121.0 (4) |
P1—Ru1—P2 | 86.35 (4) | C14A—C15A—H15A | 119.5 |
P3—Ru1—P2 | 86.97 (4) | C16A—C15A—H15A | 119.5 |
P1—Ru1—Cl3 | 91.04 (4) | C14B—C15B—C16B | 119.8 (5) |
P3—Ru1—Cl3 | 101.30 (4) | C14B—C15B—H15B | 120.1 |
P2—Ru1—Cl3 | 171.32 (4) | C16B—C15B—H15B | 120.1 |
P1—Ru1—Cl2 | 99.06 (4) | C15A—C16A—C11A | 120.1 (4) |
P3—Ru1—Cl2 | 171.32 (4) | C15A—C16A—H16A | 119.9 |
P2—Ru1—Cl2 | 94.61 (4) | C11A—C16A—H16A | 119.9 |
Cl3—Ru1—Cl2 | 77.62 (4) | C11B—C16B—C15B | 120.4 (4) |
P1—Ru1—Cl1 | 169.07 (4) | C11B—C16B—H16B | 119.8 |
P3—Ru1—Cl1 | 92.89 (4) | C15B—C16B—H16B | 119.8 |
P2—Ru1—Cl1 | 104.41 (4) | C26A—C21A—C22A | 118.8 (4) |
Cl3—Ru1—Cl1 | 78.04 (4) | C26A—C21A—P2 | 119.0 (3) |
Cl2—Ru1—Cl1 | 78.44 (4) | C22A—C21A—P2 | 122.0 (3) |
P1—Ru1—Ru2 | 124.55 (3) | C26B—C21B—C22B | 117.2 (4) |
P3—Ru1—Ru2 | 126.79 (3) | C26B—C21B—P2 | 118.1 (3) |
P2—Ru1—Ru2 | 129.45 (3) | C22B—C21B—P2 | 124.6 (3) |
Cl3—Ru1—Ru2 | 46.72 (3) | C23A—C22A—C21A | 119.4 (4) |
Cl2—Ru1—Ru2 | 46.62 (3) | C23A—C22A—H22A | 120.3 |
Cl1—Ru1—Ru2 | 46.56 (3) | C21A—C22A—H22A | 120.3 |
P4—Ru2—P6 | 89.24 (4) | C23B—C22B—C21B | 121.2 (5) |
P4—Ru2—P5 | 88.82 (5) | C23B—C22B—H22B | 119.4 |
P6—Ru2—P5 | 87.37 (4) | C21B—C22B—H22B | 119.4 |
P4—Ru2—Cl1 | 164.54 (4) | C24A—C23A—C22A | 120.8 (4) |
P6—Ru2—Cl1 | 105.98 (4) | C24A—C23A—H23A | 119.6 |
P5—Ru2—Cl1 | 89.17 (4) | C22A—C23A—H23A | 119.6 |
P4—Ru2—Cl2 | 88.08 (4) | C22B—C23B—C24B | 121.1 (5) |
P6—Ru2—Cl2 | 164.47 (4) | C22B—C23B—H23B | 119.4 |
P5—Ru2—Cl2 | 107.86 (4) | C24B—C23B—H23B | 119.4 |
Cl1—Ru2—Cl2 | 77.96 (4) | C25A—C24A—C23A | 119.6 (4) |
P4—Ru2—Cl3 | 106.14 (4) | C25A—C24A—H24A | 120.2 |
P6—Ru2—Cl3 | 89.42 (4) | C23A—C24A—H24A | 120.2 |
P5—Ru2—Cl3 | 164.66 (4) | C25B—C24B—C23B | 119.7 (5) |
Cl1—Ru2—Cl3 | 77.31 (4) | C25B—C24B—H24B | 120.1 |
Cl2—Ru2—Cl3 | 76.67 (4) | C23B—C24B—H24B | 120.1 |
P4—Ru2—Ru1 | 125.70 (3) | C24A—C25A—C26A | 120.5 (5) |
P6—Ru2—Ru1 | 126.31 (3) | C24A—C25A—H25A | 119.8 |
P5—Ru2—Ru1 | 127.00 (3) | C26A—C25A—H25A | 119.8 |
Cl1—Ru2—Ru1 | 46.39 (3) | C24B—C25B—C26B | 120.4 (5) |
Cl2—Ru2—Ru1 | 46.17 (3) | C24B—C25B—H25B | 119.8 |
Cl3—Ru2—Ru1 | 45.92 (3) | C26B—C25B—H25B | 119.8 |
Ru1—Cl1—Ru2 | 87.05 (4) | C21A—C26A—C25A | 120.7 (4) |
Ru1—Cl2—Ru2 | 87.21 (4) | C21A—C26A—H26A | 119.6 |
Ru1—Cl3—Ru2 | 87.36 (4) | C25A—C26A—H26A | 119.6 |
C11A—P1—C5 | 105.42 (17) | C21B—C26B—C25B | 120.2 (4) |
C11A—P1—C11B | 98.50 (18) | C21B—C26B—H26B | 119.9 |
C5—P1—C11B | 101.90 (18) | C25B—C26B—H26B | 119.9 |
C11A—P1—Ru1 | 115.68 (13) | C36A—C31A—C32A | 118.4 (4) |
C5—P1—Ru1 | 114.38 (12) | C36A—C31A—P3 | 118.1 (3) |
C11B—P1—Ru1 | 118.72 (13) | C32A—C31A—P3 | 123.2 (3) |
C21A—P2—C21B | 97.78 (17) | C36B—C31B—C32B | 117.4 (4) |
C21A—P2—C3 | 105.05 (17) | C36B—C31B—P3 | 120.3 (3) |
C21B—P2—C3 | 103.11 (18) | C32B—C31B—P3 | 122.3 (3) |
C21A—P2—Ru1 | 119.13 (13) | C33A—C32A—C31A | 119.7 (4) |
C21B—P2—Ru1 | 117.26 (12) | C33A—C32A—H32A | 120.1 |
C3—P2—Ru1 | 112.31 (13) | C31A—C32A—H32A | 120.1 |
C31A—P3—C4 | 104.12 (18) | C33B—C32B—C31B | 119.9 (4) |
C31A—P3—C31B | 97.36 (17) | C33B—C32B—H32B | 120.0 |
C4—P3—C31B | 102.20 (18) | C31B—C32B—H32B | 120.0 |
C31A—P3—Ru1 | 119.84 (13) | C34A—C33A—C32A | 121.2 (4) |
C4—P3—Ru1 | 112.86 (13) | C34A—C33A—H33A | 119.4 |
C31B—P3—Ru1 | 117.83 (13) | C32A—C33A—H33A | 119.4 |
C41A—P4—C41B | 98.82 (18) | C34B—C33B—C32B | 121.4 (5) |
C41A—P4—C9 | 100.36 (18) | C34B—C33B—H33B | 119.3 |
C41B—P4—C9 | 103.72 (18) | C32B—C33B—H33B | 119.3 |
C41A—P4—Ru2 | 122.27 (15) | C35A—C34A—C33A | 119.1 (4) |
C41B—P4—Ru2 | 113.97 (13) | C35A—C34A—H34A | 120.4 |
C9—P4—Ru2 | 114.91 (13) | C33A—C34A—H34A | 120.4 |
C51B—P5—C51A | 98.15 (19) | C33B—C34B—C35B | 119.2 (4) |
C51B—P5—C7 | 100.87 (19) | C33B—C34B—H34B | 120.4 |
C51A—P5—C7 | 103.86 (19) | C35B—C34B—H34B | 120.4 |
C51B—P5—Ru2 | 121.93 (15) | C36A—C35A—C34A | 121.0 (4) |
C51A—P5—Ru2 | 114.37 (14) | C36A—C35A—H35A | 119.5 |
C7—P5—Ru2 | 114.87 (13) | C34A—C35A—H35A | 119.5 |
C61B—P6—C61A | 99.37 (19) | C34B—C35B—C36B | 121.0 (5) |
C61B—P6—C8 | 103.80 (19) | C34B—C35B—H35B | 119.5 |
C61A—P6—C8 | 101.92 (18) | C36B—C35B—H35B | 119.5 |
C61B—P6—Ru2 | 113.20 (12) | C35A—C36A—C31A | 120.6 (4) |
C61A—P6—Ru2 | 120.97 (15) | C35A—C36A—H36A | 119.7 |
C8—P6—Ru2 | 115.11 (13) | C31A—C36A—H36A | 119.7 |
F3—P7—F1 | 89.8 (2) | C35B—C36B—C31B | 121.1 (4) |
F3—P7—F5 | 91.4 (3) | C35B—C36B—H36B | 119.5 |
F1—P7—F5 | 178.8 (2) | C31B—C36B—H36B | 119.5 |
F3—P7—F2 | 89.9 (2) | C42A—C41A—C46A | 118.0 (4) |
F1—P7—F2 | 90.27 (18) | C42A—C41A—P4 | 123.0 (3) |
F5—P7—F2 | 89.79 (18) | C46A—C41A—P4 | 119.0 (3) |
F3—P7—F4 | 179.0 (3) | C46B—C41B—C42B | 118.2 (4) |
F1—P7—F4 | 89.58 (19) | C46B—C41B—P4 | 123.5 (3) |
F5—P7—F4 | 89.2 (2) | C42B—C41B—P4 | 118.3 (3) |
F2—P7—F4 | 89.3 (2) | C41A—C42A—C43A | 120.2 (5) |
F3—P7—F6 | 91.4 (2) | C41A—C42A—H42A | 119.9 |
F1—P7—F6 | 90.11 (19) | C43A—C42A—H42A | 119.9 |
F5—P7—F6 | 89.8 (2) | C43B—C42B—C41B | 120.6 (5) |
F2—P7—F6 | 178.6 (2) | C43B—C42B—H42B | 119.7 |
F4—P7—F6 | 89.4 (2) | C41B—C42B—H42B | 119.7 |
C1A—O1—H1 | 109.5 | C44A—C43A—C42A | 121.9 (5) |
O1—C1A—C2A | 113.0 (5) | C44A—C43A—H43A | 119.1 |
O1—C1A—H1AA | 109.0 | C42A—C43A—H43A | 119.1 |
C2A—C1A—H1AA | 109.0 | C44B—C43B—C42B | 121.0 (5) |
O1—C1A—H1AB | 109.0 | C44B—C43B—H43B | 119.5 |
C2A—C1A—H1AB | 109.0 | C42B—C43B—H43B | 119.5 |
H1AA—C1A—H1AB | 107.8 | C43A—C44A—C45A | 118.7 (5) |
C2—C1—C4 | 108.8 (3) | C43A—C44A—H44A | 120.6 |
C2—C1—C5 | 107.5 (3) | C45A—C44A—H44A | 120.6 |
C4—C1—C5 | 110.7 (3) | C45B—C44B—C43B | 119.2 (5) |
C2—C1—C3 | 107.1 (3) | C45B—C44B—H44B | 120.4 |
C4—C1—C3 | 110.9 (3) | C43B—C44B—H44B | 120.4 |
C5—C1—C3 | 111.7 (3) | C44A—C45A—C46A | 120.8 (5) |
C1A—C2A—H2AC | 109.5 | C44A—C45A—H45A | 119.6 |
C1A—C2A—H2AB | 109.5 | C46A—C45A—H45A | 119.6 |
H2AC—C2A—H2AB | 109.5 | C44B—C45B—C46B | 120.5 (5) |
C1A—C2A—H2AA | 109.5 | C44B—C45B—H45B | 119.8 |
H2AC—C2A—H2AA | 109.5 | C46B—C45B—H45B | 119.8 |
H2AB—C2A—H2AA | 109.5 | C45A—C46A—C41A | 120.5 (5) |
C1—C2—H2A | 109.5 | C45A—C46A—H46A | 119.8 |
C1—C2—H2B | 109.5 | C41A—C46A—H46A | 119.8 |
H2A—C2—H2B | 109.5 | C41B—C46B—C45B | 120.6 (4) |
C1—C2—H2C | 109.5 | C41B—C46B—H46B | 119.7 |
H2A—C2—H2C | 109.5 | C45B—C46B—H46B | 119.7 |
H2B—C2—H2C | 109.5 | C56A—C51A—C52A | 118.4 (4) |
C1—C3—P2 | 115.2 (3) | C56A—C51A—P5 | 123.2 (3) |
C1—C3—H3A | 108.5 | C52A—C51A—P5 | 118.4 (3) |
P2—C3—H3A | 108.5 | C52B—C51B—C56B | 119.2 (4) |
C1—C3—H3B | 108.5 | C52B—C51B—P5 | 122.6 (3) |
P2—C3—H3B | 108.5 | C56B—C51B—P5 | 118.2 (4) |
H3A—C3—H3B | 107.5 | C53A—C52A—C51A | 121.3 (4) |
C1—C4—P3 | 114.2 (3) | C53A—C52A—H52A | 119.4 |
C1—C4—H4A | 108.7 | C51A—C52A—H52A | 119.4 |
P3—C4—H4A | 108.7 | C51B—C52B—C53B | 119.1 (5) |
C1—C4—H4B | 108.7 | C51B—C52B—H52B | 120.4 |
P3—C4—H4B | 108.7 | C53B—C52B—H52B | 120.4 |
H4A—C4—H4B | 107.6 | C52A—C53A—C54A | 120.4 (5) |
C1—C5—P1 | 115.2 (2) | C52A—C53A—H53A | 119.8 |
C1—C5—H5A | 108.5 | C54A—C53A—H53A | 119.8 |
P1—C5—H5A | 108.5 | C54B—C53B—C52B | 120.9 (5) |
C1—C5—H5B | 108.5 | C54B—C53B—H53B | 119.5 |
P1—C5—H5B | 108.5 | C52B—C53B—H53B | 119.5 |
H5A—C5—H5B | 107.5 | C55A—C54A—C53A | 119.6 (4) |
C8—C6—C9 | 112.6 (3) | C55A—C54A—H54A | 120.2 |
C8—C6—C7 | 111.7 (3) | C53A—C54A—H54A | 120.2 |
C9—C6—C7 | 111.5 (3) | C55B—C54B—C53B | 120.2 (5) |
C8—C6—C10 | 107.4 (3) | C55B—C54B—H54B | 119.9 |
C9—C6—C10 | 106.3 (3) | C53B—C54B—H54B | 119.9 |
C7—C6—C10 | 107.0 (3) | C54A—C55A—C56A | 121.9 (5) |
C6—C7—P5 | 117.3 (3) | C54A—C55A—H55A | 119.1 |
C6—C7—H7A | 108.0 | C56A—C55A—H55A | 119.1 |
P5—C7—H7A | 108.0 | C54B—C55B—C56B | 120.7 (6) |
C6—C7—H7B | 108.0 | C54B—C55B—H55B | 119.6 |
P5—C7—H7B | 108.0 | C56B—C55B—H55B | 119.6 |
H7A—C7—H7B | 107.2 | C51A—C56A—C55A | 118.3 (4) |
C6—C8—P6 | 117.7 (3) | C51A—C56A—H56A | 120.8 |
C6—C8—H8A | 107.9 | C55A—C56A—H56A | 120.8 |
P6—C8—H8A | 107.9 | C55B—C56B—C51B | 119.8 (5) |
C6—C8—H8B | 107.9 | C55B—C56B—H56B | 120.1 |
P6—C8—H8B | 107.9 | C51B—C56B—H56B | 120.1 |
H8A—C8—H8B | 107.2 | C62A—C61A—C66A | 118.7 (4) |
C6—C9—P4 | 117.5 (3) | C62A—C61A—P6 | 123.3 (3) |
C6—C9—H9A | 107.9 | C66A—C61A—P6 | 118.0 (3) |
P4—C9—H9A | 107.9 | C62B—C61B—C66B | 117.9 (4) |
C6—C9—H9B | 107.9 | C62B—C61B—P6 | 119.0 (3) |
P4—C9—H9B | 107.9 | C66B—C61B—P6 | 122.9 (3) |
H9A—C9—H9B | 107.2 | C61A—C62A—C63A | 118.8 (5) |
C6—C10—H10A | 109.5 | C61A—C62A—H62A | 120.6 |
C6—C10—H10B | 109.5 | C63A—C62A—H62A | 120.6 |
H10A—C10—H10B | 109.5 | C63B—C62B—C61B | 121.1 (5) |
C6—C10—H10C | 109.5 | C63B—C62B—H62B | 119.5 |
H10A—C10—H10C | 109.5 | C61B—C62B—H62B | 119.5 |
H10B—C10—H10C | 109.5 | C64A—C63A—C62A | 120.6 (5) |
C16A—C11A—C12A | 118.7 (4) | C64A—C63A—H63A | 119.7 |
C16A—C11A—P1 | 125.1 (3) | C62A—C63A—H63A | 119.7 |
C12A—C11A—P1 | 116.1 (3) | C62B—C63B—C64B | 120.4 (5) |
C16B—C11B—C12B | 118.0 (4) | C62B—C63B—H63B | 119.8 |
C16B—C11B—P1 | 124.0 (3) | C64B—C63B—H63B | 119.8 |
C12B—C11B—P1 | 118.0 (3) | C65A—C64A—C63A | 120.2 (5) |
C13A—C12A—C11A | 120.6 (4) | C65A—C64A—H64A | 119.9 |
C13A—C12A—H12A | 119.7 | C63A—C64A—H64A | 119.9 |
C11A—C12A—H12A | 119.7 | C63B—C64B—C65B | 120.0 (5) |
C13B—C12B—C11B | 121.8 (4) | C63B—C64B—H64B | 120.0 |
C13B—C12B—H12B | 119.1 | C65B—C64B—H64B | 120.0 |
C11B—C12B—H12B | 119.1 | C64A—C65A—C66A | 119.6 (5) |
C12A—C13A—C14A | 119.8 (4) | C64A—C65A—H65A | 120.2 |
C12A—C13A—H13A | 120.1 | C66A—C65A—H65A | 120.2 |
C14A—C13A—H13A | 120.1 | C64B—C65B—C66B | 119.6 (5) |
C14B—C13B—C12B | 120.3 (4) | C64B—C65B—H65B | 120.2 |
C14B—C13B—H13B | 119.8 | C66B—C65B—H65B | 120.2 |
C12B—C13B—H13B | 119.8 | C65A—C66A—C61A | 122.2 (5) |
C15A—C14A—C13A | 119.7 (4) | C65A—C66A—H66A | 118.9 |
C15A—C14A—H14A | 120.1 | C61A—C66A—H66A | 118.9 |
C13A—C14A—H14A | 120.1 | C65B—C66B—C61B | 121.0 (5) |
C13B—C14B—C15B | 119.5 (4) | C65B—C66B—H66B | 119.5 |
C13B—C14B—H14B | 120.2 | C61B—C66B—H66B | 119.5 |
C15B—C14B—H14B | 120.2 | ||
P1—Ru1—Ru2—P4 | −25.53 (5) | Ru1—P1—C5—C1 | 26.6 (3) |
P3—Ru1—Ru2—P4 | −145.74 (5) | C8—C6—C7—P5 | 56.3 (4) |
P2—Ru1—Ru2—P4 | 92.27 (5) | C9—C6—C7—P5 | −70.7 (4) |
Cl3—Ru1—Ru2—P4 | −77.34 (5) | C10—C6—C7—P5 | 173.5 (3) |
Cl2—Ru1—Ru2—P4 | 41.66 (5) | C51B—P5—C7—C6 | 145.2 (3) |
Cl1—Ru1—Ru2—P4 | 162.67 (5) | C51A—P5—C7—C6 | −113.5 (3) |
P1—Ru1—Ru2—P6 | 94.99 (5) | Ru2—P5—C7—C6 | 12.1 (4) |
P3—Ru1—Ru2—P6 | −25.22 (5) | C9—C6—C8—P6 | 57.4 (4) |
P2—Ru1—Ru2—P6 | −147.21 (5) | C7—C6—C8—P6 | −69.0 (4) |
Cl3—Ru1—Ru2—P6 | 43.18 (5) | C10—C6—C8—P6 | 174.1 (3) |
Cl2—Ru1—Ru2—P6 | 162.18 (5) | C61B—P6—C8—C6 | −115.0 (3) |
Cl1—Ru1—Ru2—P6 | −76.81 (5) | C61A—P6—C8—C6 | 142.1 (3) |
P1—Ru1—Ru2—P5 | −146.17 (5) | Ru2—P6—C8—C6 | 9.3 (3) |
P3—Ru1—Ru2—P5 | 93.62 (5) | C8—C6—C9—P4 | −69.2 (4) |
P2—Ru1—Ru2—P5 | −28.37 (5) | C7—C6—C9—P4 | 57.3 (4) |
Cl3—Ru1—Ru2—P5 | 162.02 (5) | C10—C6—C9—P4 | 173.5 (3) |
Cl2—Ru1—Ru2—P5 | −78.98 (5) | C41A—P4—C9—C6 | 143.6 (3) |
Cl1—Ru1—Ru2—P5 | 42.03 (5) | C41B—P4—C9—C6 | −114.6 (3) |
P1—Ru1—Ru2—Cl1 | 171.80 (5) | Ru2—P4—C9—C6 | 10.5 (4) |
P3—Ru1—Ru2—Cl1 | 51.59 (5) | C5—P1—C11A—C16A | −13.4 (4) |
P2—Ru1—Ru2—Cl1 | −70.40 (5) | C11B—P1—C11A—C16A | −118.3 (4) |
Cl3—Ru1—Ru2—Cl1 | 119.99 (5) | Ru1—P1—C11A—C16A | 114.1 (3) |
Cl2—Ru1—Ru2—Cl1 | −121.01 (5) | C5—P1—C11A—C12A | 165.8 (3) |
P1—Ru1—Ru2—Cl2 | −67.19 (5) | C11B—P1—C11A—C12A | 60.9 (3) |
P3—Ru1—Ru2—Cl2 | 172.60 (5) | Ru1—P1—C11A—C12A | −66.7 (3) |
P2—Ru1—Ru2—Cl2 | 50.61 (5) | C11A—P1—C11B—C16B | −134.9 (4) |
Cl3—Ru1—Ru2—Cl2 | −119.00 (5) | C5—P1—C11B—C16B | 117.2 (4) |
Cl1—Ru1—Ru2—Cl2 | 121.01 (5) | Ru1—P1—C11B—C16B | −9.4 (4) |
P1—Ru1—Ru2—Cl3 | 51.80 (5) | C11A—P1—C11B—C12B | 45.0 (4) |
P3—Ru1—Ru2—Cl3 | −68.40 (5) | C5—P1—C11B—C12B | −62.8 (4) |
P2—Ru1—Ru2—Cl3 | 169.61 (5) | Ru1—P1—C11B—C12B | 170.6 (3) |
Cl2—Ru1—Ru2—Cl3 | 119.00 (5) | C16A—C11A—C12A—C13A | 0.4 (6) |
Cl1—Ru1—Ru2—Cl3 | −119.99 (5) | P1—C11A—C12A—C13A | −178.8 (3) |
P1—Ru1—Cl1—Ru2 | −38.3 (2) | C16B—C11B—C12B—C13B | 3.3 (7) |
P3—Ru1—Cl1—Ru2 | −141.07 (4) | P1—C11B—C12B—C13B | −176.7 (4) |
P2—Ru1—Cl1—Ru2 | 131.32 (4) | C11A—C12A—C13A—C14A | −1.4 (7) |
Cl3—Ru1—Cl1—Ru2 | −40.13 (4) | C11B—C12B—C13B—C14B | −1.8 (8) |
Cl2—Ru1—Cl1—Ru2 | 39.48 (3) | C12A—C13A—C14A—C15A | 1.6 (7) |
P4—Ru2—Cl1—Ru1 | −65.14 (15) | C12B—C13B—C14B—C15B | −1.4 (8) |
P6—Ru2—Cl1—Ru1 | 125.31 (4) | C13A—C14A—C15A—C16A | −0.8 (7) |
P5—Ru2—Cl1—Ru1 | −147.67 (4) | C13B—C14B—C15B—C16B | 3.1 (8) |
Cl2—Ru2—Cl1—Ru1 | −39.21 (4) | C14A—C15A—C16A—C11A | −0.3 (7) |
Cl3—Ru2—Cl1—Ru1 | 39.63 (3) | C12A—C11A—C16A—C15A | 0.5 (6) |
P1—Ru1—Cl2—Ru2 | 129.75 (3) | P1—C11A—C16A—C15A | 179.6 (3) |
P3—Ru1—Cl2—Ru2 | −43.1 (3) | C12B—C11B—C16B—C15B | −1.5 (7) |
P2—Ru1—Cl2—Ru2 | −143.22 (3) | P1—C11B—C16B—C15B | 178.5 (4) |
Cl3—Ru1—Cl2—Ru2 | 40.69 (3) | C14B—C15B—C16B—C11B | −1.6 (8) |
Cl1—Ru1—Cl2—Ru2 | −39.43 (3) | C21B—P2—C21A—C26A | 90.6 (4) |
P4—Ru2—Cl2—Ru1 | −147.31 (4) | C3—P2—C21A—C26A | −163.5 (3) |
P6—Ru2—Cl2—Ru1 | −67.11 (15) | Ru1—P2—C21A—C26A | −36.7 (4) |
P5—Ru2—Cl2—Ru1 | 124.55 (4) | C21B—P2—C21A—C22A | −85.6 (4) |
Cl1—Ru2—Cl2—Ru1 | 39.39 (4) | C3—P2—C21A—C22A | 20.3 (4) |
Cl3—Ru2—Cl2—Ru1 | −40.22 (4) | Ru1—P2—C21A—C22A | 147.1 (3) |
P1—Ru1—Cl3—Ru2 | −139.66 (4) | C21A—P2—C21B—C26B | −69.9 (3) |
P3—Ru1—Cl3—Ru2 | 130.59 (4) | C3—P2—C21B—C26B | −177.4 (3) |
P2—Ru1—Cl3—Ru2 | −67.3 (3) | Ru1—P2—C21B—C26B | 58.7 (3) |
Cl2—Ru1—Cl3—Ru2 | −40.60 (4) | C21A—P2—C21B—C22B | 106.4 (4) |
Cl1—Ru1—Cl3—Ru2 | 40.00 (4) | C3—P2—C21B—C22B | −1.1 (4) |
P4—Ru2—Cl3—Ru1 | 124.43 (4) | Ru1—P2—C21B—C22B | −125.0 (3) |
P6—Ru2—Cl3—Ru1 | −146.53 (4) | C26A—C21A—C22A—C23A | 2.9 (7) |
P5—Ru2—Cl3—Ru1 | −68.69 (15) | P2—C21A—C22A—C23A | 179.1 (4) |
Cl1—Ru2—Cl3—Ru1 | −40.00 (3) | C26B—C21B—C22B—C23B | −4.1 (6) |
Cl2—Ru2—Cl3—Ru1 | 40.42 (3) | P2—C21B—C22B—C23B | 179.6 (3) |
P3—Ru1—P1—C11A | −176.72 (15) | C21A—C22A—C23A—C24A | −0.8 (8) |
P2—Ru1—P1—C11A | −89.73 (15) | C21B—C22B—C23B—C24B | 0.5 (7) |
Cl3—Ru1—P1—C11A | 81.99 (15) | C22A—C23A—C24A—C25A | −2.3 (9) |
Cl2—Ru1—P1—C11A | 4.36 (15) | C22B—C23B—C24B—C25B | 2.3 (8) |
Cl1—Ru1—P1—C11A | 80.2 (3) | C23A—C24A—C25A—C26A | 3.1 (8) |
Ru2—Ru1—P1—C11A | 47.08 (15) | C23B—C24B—C25B—C26B | −1.4 (7) |
P3—Ru1—P1—C5 | −53.92 (15) | C22A—C21A—C26A—C25A | −2.1 (7) |
P2—Ru1—P1—C5 | 33.08 (15) | P2—C21A—C26A—C25A | −178.4 (4) |
Cl3—Ru1—P1—C5 | −155.21 (15) | C24A—C25A—C26A—C21A | −0.9 (8) |
Cl2—Ru1—P1—C5 | 127.16 (15) | C22B—C21B—C26B—C25B | 4.9 (6) |
Cl1—Ru1—P1—C5 | −157.0 (2) | P2—C21B—C26B—C25B | −178.6 (3) |
Ru2—Ru1—P1—C5 | 169.89 (14) | C24B—C25B—C26B—C21B | −2.3 (7) |
P3—Ru1—P1—C11B | 66.51 (15) | C4—P3—C31A—C36A | −175.3 (3) |
P2—Ru1—P1—C11B | 153.50 (15) | C31B—P3—C31A—C36A | 80.1 (4) |
Cl3—Ru1—P1—C11B | −34.78 (15) | Ru1—P3—C31A—C36A | −48.0 (4) |
Cl2—Ru1—P1—C11B | −112.41 (15) | C4—P3—C31A—C32A | 11.3 (4) |
Cl1—Ru1—P1—C11B | −36.5 (3) | C31B—P3—C31A—C32A | −93.3 (4) |
Ru2—Ru1—P1—C11B | −69.69 (15) | Ru1—P3—C31A—C32A | 138.6 (3) |
P1—Ru1—P2—C21A | 175.35 (15) | C31A—P3—C31B—C36B | 61.2 (4) |
P3—Ru1—P2—C21A | −94.91 (15) | C4—P3—C31B—C36B | −45.0 (4) |
Cl3—Ru1—P2—C21A | 102.7 (3) | Ru1—P3—C31B—C36B | −169.3 (3) |
Cl2—Ru1—P2—C21A | 76.53 (15) | C31A—P3—C31B—C32B | −117.8 (4) |
Cl1—Ru1—P2—C21A | −2.70 (15) | C4—P3—C31B—C32B | 136.0 (4) |
Ru2—Ru1—P2—C21A | 42.23 (16) | Ru1—P3—C31B—C32B | 11.7 (4) |
P1—Ru1—P2—C21B | 57.87 (15) | C36A—C31A—C32A—C33A | −0.9 (6) |
P3—Ru1—P2—C21B | 147.62 (15) | P3—C31A—C32A—C33A | 172.5 (3) |
Cl3—Ru1—P2—C21B | −14.8 (3) | C36B—C31B—C32B—C33B | −0.3 (6) |
Cl2—Ru1—P2—C21B | −40.94 (15) | P3—C31B—C32B—C33B | 178.8 (4) |
Cl1—Ru1—P2—C21B | −120.17 (15) | C31A—C32A—C33A—C34A | 1.3 (7) |
Ru2—Ru1—P2—C21B | −75.24 (15) | C31B—C32B—C33B—C34B | 0.8 (8) |
P1—Ru1—P2—C3 | −61.29 (13) | C32A—C33A—C34A—C35A | −0.9 (7) |
P3—Ru1—P2—C3 | 28.45 (13) | C32B—C33B—C34B—C35B | −1.4 (8) |
Cl3—Ru1—P2—C3 | −134.0 (3) | C33A—C34A—C35A—C36A | 0.2 (8) |
Cl2—Ru1—P2—C3 | −160.11 (13) | C33B—C34B—C35B—C36B | 1.5 (8) |
Cl1—Ru1—P2—C3 | 120.66 (13) | C34A—C35A—C36A—C31A | 0.2 (8) |
Ru2—Ru1—P2—C3 | 165.59 (12) | C32A—C31A—C36A—C35A | 0.2 (7) |
P1—Ru1—P3—C31A | −97.72 (14) | P3—C31A—C36A—C35A | −173.5 (4) |
P2—Ru1—P3—C31A | 175.91 (14) | C34B—C35B—C36B—C31B | −1.1 (8) |
Cl3—Ru1—P3—C31A | −6.75 (15) | C32B—C31B—C36B—C35B | 0.4 (7) |
Cl2—Ru1—P3—C31A | 75.2 (3) | P3—C31B—C36B—C35B | −178.7 (4) |
Cl1—Ru1—P3—C31A | 71.63 (15) | C41B—P4—C41A—C42A | 129.2 (4) |
Ru2—Ru1—P3—C31A | 36.90 (15) | C9—P4—C41A—C42A | −125.0 (4) |
P1—Ru1—P3—C4 | 25.44 (14) | Ru2—P4—C41A—C42A | 3.4 (4) |
P2—Ru1—P3—C4 | −60.92 (14) | C41B—P4—C41A—C46A | −51.0 (4) |
Cl3—Ru1—P3—C4 | 116.41 (14) | C9—P4—C41A—C46A | 54.8 (4) |
Cl2—Ru1—P3—C4 | −161.6 (3) | Ru2—P4—C41A—C46A | −176.8 (3) |
Cl1—Ru1—P3—C4 | −165.21 (14) | C41A—P4—C41B—C46B | 135.2 (4) |
Ru2—Ru1—P3—C4 | 160.06 (14) | C9—P4—C41B—C46B | 32.1 (4) |
P1—Ru1—P3—C31B | 144.25 (14) | Ru2—P4—C41B—C46B | −93.5 (4) |
P2—Ru1—P3—C31B | 57.89 (14) | C41A—P4—C41B—C42B | −45.7 (4) |
Cl3—Ru1—P3—C31B | −124.78 (14) | C9—P4—C41B—C42B | −148.7 (3) |
Cl2—Ru1—P3—C31B | −42.8 (3) | Ru2—P4—C41B—C42B | 85.6 (3) |
Cl1—Ru1—P3—C31B | −46.40 (14) | C46A—C41A—C42A—C43A | −0.2 (6) |
Ru2—Ru1—P3—C31B | −81.13 (14) | P4—C41A—C42A—C43A | 179.6 (3) |
P6—Ru2—P4—C41A | −83.43 (15) | C46B—C41B—C42B—C43B | 1.4 (7) |
P5—Ru2—P4—C41A | −170.81 (15) | P4—C41B—C42B—C43B | −177.7 (4) |
Cl1—Ru2—P4—C41A | 106.6 (2) | C41A—C42A—C43A—C44A | −0.3 (7) |
Cl2—Ru2—P4—C41A | 81.28 (15) | C41B—C42B—C43B—C44B | −0.2 (8) |
Cl3—Ru2—P4—C41A | 5.75 (16) | C42A—C43A—C44A—C45A | 0.7 (8) |
Ru1—Ru2—P4—C41A | 52.61 (16) | C42B—C43B—C44B—C45B | −1.3 (8) |
P6—Ru2—P4—C41B | 157.94 (15) | C43A—C44A—C45A—C46A | −0.6 (8) |
P5—Ru2—P4—C41B | 70.56 (15) | C43B—C44B—C45B—C46B | 1.5 (8) |
Cl1—Ru2—P4—C41B | −12.0 (2) | C44A—C45A—C46A—C41A | 0.2 (8) |
Cl2—Ru2—P4—C41B | −37.35 (15) | C42A—C41A—C46A—C45A | 0.2 (7) |
Cl3—Ru2—P4—C41B | −112.88 (15) | P4—C41A—C46A—C45A | −179.6 (4) |
Ru1—Ru2—P4—C41B | −66.02 (15) | C42B—C41B—C46B—C45B | −1.3 (6) |
P6—Ru2—P4—C9 | 38.43 (15) | P4—C41B—C46B—C45B | 177.9 (3) |
P5—Ru2—P4—C9 | −48.95 (15) | C44B—C45B—C46B—C41B | −0.2 (7) |
Cl1—Ru2—P4—C9 | −131.53 (19) | C51B—P5—C51A—C56A | 130.2 (4) |
Cl2—Ru2—P4—C9 | −156.87 (15) | C7—P5—C51A—C56A | 26.8 (4) |
Cl3—Ru2—P4—C9 | 127.60 (15) | Ru2—P5—C51A—C56A | −99.2 (4) |
Ru1—Ru2—P4—C9 | 174.46 (14) | C51B—P5—C51A—C52A | −52.5 (4) |
P4—Ru2—P5—C51B | −83.87 (16) | C7—P5—C51A—C52A | −155.9 (3) |
P6—Ru2—P5—C51B | −173.17 (16) | Ru2—P5—C51A—C52A | 78.2 (3) |
Cl1—Ru2—P5—C51B | 80.80 (16) | C51A—P5—C51B—C52B | 128.1 (4) |
Cl2—Ru2—P5—C51B | 3.73 (17) | C7—P5—C51B—C52B | −126.0 (4) |
Cl3—Ru2—P5—C51B | 108.7 (2) | Ru2—P5—C51B—C52B | 2.7 (4) |
Ru1—Ru2—P5—C51B | 51.79 (17) | C51A—P5—C51B—C56B | −52.6 (4) |
P4—Ru2—P5—C51A | 158.37 (16) | C7—P5—C51B—C56B | 53.3 (4) |
P6—Ru2—P5—C51A | 69.08 (16) | Ru2—P5—C51B—C56B | −178.1 (3) |
Cl1—Ru2—P5—C51A | −36.96 (16) | C56A—C51A—C52A—C53A | 1.3 (7) |
Cl2—Ru2—P5—C51A | −114.02 (16) | P5—C51A—C52A—C53A | −176.1 (4) |
Cl3—Ru2—P5—C51A | −9.0 (2) | C56B—C51B—C52B—C53B | −1.0 (7) |
Ru1—Ru2—P5—C51A | −65.96 (16) | P5—C51B—C52B—C53B | 178.2 (4) |
P4—Ru2—P5—C7 | 38.39 (16) | C51A—C52A—C53A—C54A | −0.2 (7) |
P6—Ru2—P5—C7 | −50.90 (16) | C51B—C52B—C53B—C54B | 0.9 (8) |
Cl1—Ru2—P5—C7 | −156.94 (16) | C52A—C53A—C54A—C55A | −2.0 (8) |
Cl2—Ru2—P5—C7 | 125.99 (15) | C52B—C53B—C54B—C55B | 0.7 (9) |
Cl3—Ru2—P5—C7 | −129.01 (19) | C53A—C54A—C55A—C56A | 3.0 (8) |
Ru1—Ru2—P5—C7 | 174.06 (15) | C53B—C54B—C55B—C56B | −2.2 (9) |
P4—Ru2—P6—C61B | 71.35 (17) | C52A—C51A—C56A—C55A | −0.4 (6) |
P5—Ru2—P6—C61B | 160.20 (17) | P5—C51A—C56A—C55A | 177.0 (3) |
Cl1—Ru2—P6—C61B | −111.42 (17) | C54A—C55A—C56A—C51A | −1.8 (7) |
Cl2—Ru2—P6—C61B | −8.7 (2) | C54B—C55B—C56B—C51B | 2.0 (9) |
Cl3—Ru2—P6—C61B | −34.81 (17) | C52B—C51B—C56B—C55B | −0.4 (7) |
Ru1—Ru2—P6—C61B | −64.26 (17) | P5—C51B—C56B—C55B | −179.6 (4) |
P4—Ru2—P6—C61A | −171.01 (15) | C61B—P6—C61A—C62A | 124.2 (4) |
P5—Ru2—P6—C61A | −82.16 (15) | C8—P6—C61A—C62A | −129.5 (4) |
Cl1—Ru2—P6—C61A | 6.22 (15) | Ru2—P6—C61A—C62A | −0.2 (4) |
Cl2—Ru2—P6—C61A | 108.95 (19) | C61B—P6—C61A—C66A | −55.2 (4) |
Cl3—Ru2—P6—C61A | 82.83 (15) | C8—P6—C61A—C66A | 51.2 (4) |
Ru1—Ru2—P6—C61A | 53.38 (15) | Ru2—P6—C61A—C66A | −179.6 (3) |
P4—Ru2—P6—C8 | −47.83 (14) | C61A—P6—C61B—C62B | −50.6 (3) |
P5—Ru2—P6—C8 | 41.02 (14) | C8—P6—C61B—C62B | −155.4 (3) |
Cl1—Ru2—P6—C8 | 129.40 (14) | Ru2—P6—C61B—C62B | 79.1 (3) |
Cl2—Ru2—P6—C8 | −127.87 (19) | C61A—P6—C61B—C66B | 134.0 (3) |
Cl3—Ru2—P6—C8 | −153.98 (14) | C8—P6—C61B—C66B | 29.2 (4) |
Ru1—Ru2—P6—C8 | 176.57 (13) | Ru2—P6—C61B—C66B | −96.3 (3) |
C2—C1—C3—P2 | 159.4 (3) | C66A—C61A—C62A—C63A | 1.6 (6) |
C4—C1—C3—P2 | −82.0 (3) | P6—C61A—C62A—C63A | −177.8 (3) |
C5—C1—C3—P2 | 42.0 (4) | C66B—C61B—C62B—C63B | −0.3 (6) |
C21A—P2—C3—C1 | 164.3 (3) | P6—C61B—C62B—C63B | −175.9 (3) |
C21B—P2—C3—C1 | −93.8 (3) | C61A—C62A—C63A—C64A | −0.6 (7) |
Ru1—P2—C3—C1 | 33.3 (3) | C61B—C62B—C63B—C64B | 0.7 (7) |
C2—C1—C4—P3 | 158.9 (3) | C62A—C63A—C64A—C65A | −0.3 (8) |
C5—C1—C4—P3 | −83.2 (3) | C62B—C63B—C64B—C65B | −1.3 (7) |
C3—C1—C4—P3 | 41.3 (4) | C63A—C64A—C65A—C66A | 0.1 (8) |
C31A—P3—C4—C1 | 166.2 (3) | C63B—C64B—C65B—C66B | 1.6 (7) |
C31B—P3—C4—C1 | −92.9 (3) | C64A—C65A—C66A—C61A | 1.0 (8) |
Ru1—P3—C4—C1 | 34.7 (3) | C62A—C61A—C66A—C65A | −1.8 (7) |
C2—C1—C5—P1 | 165.8 (3) | P6—C61A—C66A—C65A | 177.5 (4) |
C4—C1—C5—P1 | 47.1 (4) | C64B—C65B—C66B—C61B | −1.2 (7) |
C3—C1—C5—P1 | −77.0 (4) | C62B—C61B—C66B—C65B | 0.6 (6) |
C11A—P1—C5—C1 | 154.8 (3) | P6—C61B—C66B—C65B | 176.0 (3) |
C11B—P1—C5—C1 | −102.8 (3) |
Experimental details
Crystal data | |
Chemical formula | [Ru2Cl3(C41H39P3)2]PF6·C2H6O |
Mr | 1748.79 |
Crystal system, space group | Monoclinic, Cc |
Temperature (K) | 293 |
a, b, c (Å) | 13.069 (3), 25.602 (5), 22.991 (5) |
β (°) | 92.66 (3) |
V (Å3) | 7684 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.71 |
Crystal size (mm) | 0.20 × 0.12 × 0.09 |
Data collection | |
Diffractometer | Stoe IPDS area-detector diffractometer |
Absorption correction | Numerical (X-RED; Stoe & Cie, 1997) |
Tmin, Tmax | 0.908, 0.959 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 26982, 14149, 11740 |
Rint | 0.039 |
(sin θ/λ)max (Å−1) | 0.613 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.033, 0.057, 0.89 |
No. of reflections | 14149 |
No. of parameters | 933 |
No. of restraints | 3 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.39, −0.59 |
Absolute structure | Flack (1983), with 6746 Friedel pairs |
Absolute structure parameter | 0.725 (17) |
Computer programs: IPDS (Stoe & Cie, 1997), IPDS, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 1996).
Ru1—P1 | 2.2469 (11) | Ru2—P4 | 2.2617 (12) |
Ru1—P3 | 2.2682 (12) | Ru2—P6 | 2.2635 (11) |
Ru1—P2 | 2.2719 (11) | Ru2—P5 | 2.2657 (11) |
Ru1—Cl3 | 2.4449 (12) | Ru2—Cl1 | 2.4717 (12) |
Ru1—Cl2 | 2.4553 (13) | Ru2—Cl2 | 2.4738 (11) |
Ru1—Cl1 | 2.4650 (12) | Ru2—Cl3 | 2.4776 (12) |
Ru1—Ru2 | 3.3997 (7) | ||
P1—Ru1—P3 | 89.55 (4) | P6—Ru2—P5 | 87.37 (4) |
P1—Ru1—P2 | 86.35 (4) | Cl1—Ru2—Cl2 | 77.96 (4) |
P3—Ru1—P2 | 86.97 (4) | Cl1—Ru2—Cl3 | 77.31 (4) |
Cl3—Ru1—Cl2 | 77.62 (4) | Cl2—Ru2—Cl3 | 76.67 (4) |
Cl3—Ru1—Cl1 | 78.04 (4) | Ru1—Cl1—Ru2 | 87.05 (4) |
Cl2—Ru1—Cl1 | 78.44 (4) | Ru1—Cl2—Ru2 | 87.21 (4) |
P4—Ru2—P6 | 89.24 (4) | Ru1—Cl3—Ru2 | 87.36 (4) |
P4—Ru2—P5 | 88.82 (5) |
Complexes of rhodium and ruthenium with optically active ligands are widely used as catalysts for enantioselective hydrogenation reactions (Chen et al., 1999; Oketa et al., 1999). While looking for related complexes suitable as catalysts for oxidation processes, we noted that Ru complexes with aryl phosphine ligands are not well described in the literature (Barbaro et al., 1999). In comparison, there are extensive studies of the redox chemistry of oxo and nitrido Ru or Os complexes containing polypyridine, Schiff base or porphyrin ligands (Lebeau et al., 2001). Such complexes are supposed to act as oxidants in metal-catalyzed oxidation reactions.
Generally, six-coordinated RuIV oxo complexes are prepared starting from the related RuII chloro species via the corresponding RuII aquo complexes, which are finally oxidized (Navarro et al., 1998). In order to extend this synthesis to analogous Ru complexes with phosphine ligands, we attempted to prepare the chloro complex [Ru(tripod)(dppb)Cl][PF6] by reaction of [RuIII(tripod)Cl3] [tripod is 1,1,1-tris(diphenylphosphinomethyl)ethane; Ott et al., 1985] with dppb [1,4-bis(diphenylphosphino)butane] and subsequent precipitation with NH4PF6. However, instead of the expected mononuclear chloro complex, the dinuclear trichloro-bridged ethanol-solvated complex [Ru2(µ-Cl)3(tripod)2][PF6]·C2H6O, (I), was obtained in the form of yellow crystals. Obviously, dppb acts here only as a reducing agent providing two electrons, and does not coordinate to the Ru atom. The identity of the new complex is indicated by multinuclear NMR, IR and UV data and is confirmed by the results of a single-crystal X-ray structure determination, which are presented here. \sch
The crystal of (I) consists of discrete [Ru2(µ-Cl)3(tripod)2]+ cations and [PF6]− anions and contains one molecule of ethanol in the molecular unit (Fig. 1). Each Ru atom is coordinated by the three bridging Cl atoms and by the three P atoms of the tripod ligand in a slightly distorted octahedral environment. In the dinuclear unit, two such octahedra share a common face, with the bridging Cl atoms occupying its edges. The two P3Ru fragments are exactly eclipsed, while the bridging Cl atoms are staggered with respect to the six P atoms (Fig. 2).
The bond distances and angles of the dinuclear cation in (I) compare well with those of the corresponding tetraphenyloborate salt reported by Rhodes et al. (1988), indicating only a small counterion effect. The Ru—P [2.246 (1)–2.272 (1) Å] and Ru—Cl distances [2.445 (1)–2.478 (1) Å] in the hexafluorophosphate, (I), are slightly shorter than those found for the tetraphenyloborate. The Ru—Cl—Ru bond angles of about 87° are larger than those calculated for an ideal cofacial bioctahedral geometry (75.0°). Accordingly, the Cl—Ru—Cl bond angles of about 78° are smaller than the ideal value of 90°. This results in an elongation of the bioctahedron along the Ru···Ru axis and thus in a longer Ru···Ru distance [3.3997 (7) Å] than would be expected for a regular face-sharing bioctahedron, excluding a bond interaction between the two Ru atoms. The P—Ru—P bond angles are between 86.35 (4) and 89.59 (4)°, comparable with those found for complexes with tridentate phosphine ligands (Pal & Pal, 2001) and smaller than those in related complexes with monodentate phosphine ligands (Higham et al., 1998; Laing & Pope, 1976; Rhodes et al., 1988).
As is generally found for tripod complexes, the bond lengths and angles of the tripod ligand in (I) deviate only slightly from those observed for the free ligand (Bianchini et al., 1982). The tetracoordinated P atoms display a distorted tetrahedral coordination, with Ru—P—Caryl 113.24 (12)–122.23 (15), Ru—P—Calkyl 112.28 (13)–115.10 (14), Calkyl—P—Caryl 100.16 (19)–105.64 (19) and Caryl—P—Caryl 97.34 (17)–99.33 (19)°. The bond lengths and angles in the hexafluorophosphate anion are as expected.